A porous metal-organic framework[C21H20CoF6O7]was synthesized with Co(CH3COO)2·4H2O and CPHFP(2,2'-bis(4-carboxyphenyl)hexafluoro-propane)under hydrothermal conditions.This FMOF-Co has been characterized by elemental analysis,infrared spectroscopy,thermogravimetric analysis,single-crystal and powder X-ray diffraction.The crystal is of monoclinic space group P21/n with a = 7.8911(2),b = 29.9053(8),c =10.5811(3)?,β = 90.193(10)°,V = 2499.70(12)?3,Z = 4,Mr = 557.3,Dc = 1.481 g·cm-3,F(000)= 1132,μ =0.768 mm-1,GOOF = 1.035,the final R = 0.0722 and wR = 0.2326 for 6347 observed reflections with Ⅰ>2a(Ⅰ).The structure of FMOF-Co is constructed form the linkage of Co(Ⅱ)through CPHFP,forming a 3D net framework.The Kr and Xe uptake values are 0.225 and 0.484 mmol·g-1 at 303 K(100 KPa)with their mol selectivity to be 0.46;while the Kr and Xe uptake values are 0.486 and 0.077 mmol·g-1 at 233 K(100 KPa),with their mol separation being 6.29 at this condition.